US9383314B2 - Maturation apparatus and methods - Google Patents

Maturation apparatus and methods Download PDF

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US9383314B2
US9383314B2 US14/232,030 US201214232030A US9383314B2 US 9383314 B2 US9383314 B2 US 9383314B2 US 201214232030 A US201214232030 A US 201214232030A US 9383314 B2 US9383314 B2 US 9383314B2
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vessel
cask
light source
monitoring
maturation process
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US20140160465A1 (en
Inventor
Graeme P. Malcolm
Gareth T. Maker
Gordon Robertson
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M Squared Lasers Ltd
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M Squared Lasers Ltd
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Assigned to M SQUARED LASERS LIMITED reassignment M SQUARED LASERS LIMITED ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: MALCOLM, GRAEME, MAKER, GARETH, ROBERTSON, GORDON
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    • C—CHEMISTRY; METALLURGY
    • C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12G—WINE; PREPARATION THEREOF; ALCOHOLIC BEVERAGES; PREPARATION OF ALCOHOLIC BEVERAGES NOT PROVIDED FOR IN SUBCLASSES C12C OR C12H
    • C12G3/00—Preparation of other alcoholic beverages
    • C12G3/08—Preparation of other alcoholic beverages by methods for altering the composition of fermented solutions or alcoholic beverages not provided for in groups C12G3/02 - C12G3/07
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/59—Transmissivity
    • C—CHEMISTRY; METALLURGY
    • C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12H—PASTEURISATION, STERILISATION, PRESERVATION, PURIFICATION, CLARIFICATION OR AGEING OF ALCOHOLIC BEVERAGES; METHODS FOR ALTERING THE ALCOHOL CONTENT OF FERMENTED SOLUTIONS OR ALCOHOLIC BEVERAGES
    • C12H1/00—Pasteurisation, sterilisation, preservation, purification, clarification, or ageing of alcoholic beverages
    • C12H1/22—Ageing or ripening by storing, e.g. lagering of beer
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
    • G01N21/3504—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing gases, e.g. multi-gas analysis
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
    • G01N21/3504—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing gases, e.g. multi-gas analysis
    • G01N2021/3513—Open path with an instrumental source
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2201/00—Features of devices classified in G01N21/00
    • G01N2201/02—Mechanical
    • G01N2201/022—Casings
    • G01N2201/0227—Sealable enclosure

Definitions

  • the present invention relates to apparatus and methods for use in maturation processes, and in particular apparatus and methods for reducing fluid loss from a cask during a maturation process, and apparatus and methods for controlling and for monitoring a maturation process.
  • a particular embodiment provides a vessel to sealably enclose the cask and provide an expansion volume to receive fluid vapour from the cask.
  • Scotch malt whisky production involves several stages, the most important of which is arguably the maturation process by which new-make whisky is matured for several years in wooden casks.
  • Whisky is typically ⁇ 60% water, ⁇ 40% ethanol (and ⁇ 0.1% other constituents), when it is casked, but during the maturation process (which typically takes ten to twenty years) a proportion of the fluid volume in the cask is lost to the atmosphere. This is affectionately referred to in the trade as the “angels' share”.
  • the angels' share is, in Scotland, typically around 2% volume per annum. Elsewhere in the world the loss can be as high as 5% per annum. Some whisky producers may have tens of millions of whisky casks undergoing maturation at any one time so these losses are clearly significant.
  • an apparatus to reduce fluid loss from a cask during a maturation process comprising a vessel to sealably enclose the cask and provide an expansion volume to receive fluid vapour from the cask.
  • whisky casks leak ethanol vapour to the surrounding environment.
  • ethanol vapour is initially able to leave the cask until the partial pressure of ethanol vapour (or other fluid lost from the cask) within the vessel reaches an equilibrium value at which there will be no further leakage.
  • the apparatus further comprises a monitoring system arranged to monitor the presence of fluid vapour within the vessel.
  • the monitoring system permits monitoring of the leak rate as a function of time.
  • the monitoring system comprises a light source and a detector, the detector arranged to receive light from the light source and the monitoring system configured to determine a relative transmission of the light through the vessel.
  • the apparatus comprises at least one aperture in a wall of the vessel, the light source and detector arranged on opposite sides of the aperture.
  • the apparatus comprises two apertures located in walls of the vessel and defining an optical path through the vessel intersecting the light source and the detector.
  • the apparatus further comprises a mirror arranged to receive and reflect light from the light source to the detector via a same aperture.
  • the at least one aperture comprises a window.
  • the window may comprise calcium fluoride (CaF 2 ).
  • the light source comprises a laser source.
  • the light source comprises an infrared laser source.
  • the light source comprises an optical parametric oscillator mid-infrared source.
  • the light source comprises a quantum cascade laser source.
  • the light source may be tuned to an absorption line or absorption band of ethanol.
  • the monitoring system comprises an active infrared hyperspectral imaging system.
  • the vessel comprises a lid.
  • the lid and/or main body of the vessel may be provided with a rubber gasket or O-ring to provide a seal there between.
  • the vessel is rectangular.
  • the vessel is cylindrical or cask-shaped.
  • the vessel is sized to receive a plurality of casks.
  • the vessel is in fluid communication with one or more like vessels with or without respective monitoring systems.
  • a method of reducing fluid loss from a cask during a maturation process comprising sealing the cask within a vessel having an expansion volume, and receiving fluid vapour from the cask in the expansion volume of the vessel.
  • the method further comprises monitoring the presence of ethanol within the sealed vessel.
  • the method further comprises monitoring the presence of water vapour within the sealed vessel.
  • the method comprises obtaining a background measurement of the presence of ethanol within the sealed vessel.
  • the method comprises recording the presence of ethanol within the sealed vessel as a function of time.
  • Embodiments of the second aspect of the invention may include one or more features corresponding to features of the first aspect of the invention or its embodiments, or vice versa.
  • a monitoring system to monitor fluid loss from a cask during a maturation process, the monitoring system comprising a light source and a detector, the detector arranged to receive light from the light source and the monitoring system arranged to determine the presence of fluid vapour in the vicinity of the cask.
  • the light source comprises a laser source.
  • the light source comprises an optical parametric oscillator mid-infrared source.
  • the light source comprises a quantum cascade laser source.
  • the light source may be tuned to an absorption line or absorption band of ethanol.
  • Embodiments of the third aspect of the invention may include one or more features corresponding to features of the first or second aspects of the invention or its embodiments, or vice versa.
  • a method of monitoring fluid loss from a cask during a maturation process comprising emitting light from a light source, receiving light from the light source at a detector, and determining a relative transmission of the light in the vicinity of the cask.
  • the method comprises locating one or both of the light source and detector proximal to the cask.
  • Embodiments of the fourth aspect of the invention may include one or more features corresponding to features of the first, second or third aspects of the invention or its embodiments, or vice versa.
  • a system for controlling a maturation process comprising the apparatus of the first aspect and a control system configured to control environmental conditions within the sealed vessel.
  • the vessel is sized to provide sufficient atmospheric oxygen for at least a portion of the maturation process.
  • the vessel is sized to provide sufficient water vapour for at least a portion of the maturation process.
  • the system comprises at least one pump operable to control an ambient pressure within the vessel.
  • the pump is operable to maintain a target ambient pressure within the vessel.
  • the system comprises one or more gas sources in fluid communication with the vessel, operable to control the presence of one or more gases within the vessel.
  • the system further comprises one or more heating and/or cooling devices configured to control a temperature of the vessel.
  • Embodiments of the fifth aspect of the invention may include one or more features corresponding to features of the first to fourth aspects of the invention or its embodiments, or vice versa.
  • a method of controlling a cask maturation process comprising sealing the cask within a vessel, and controlling environmental conditions within the sealed vessel.
  • the method comprises controlling the temperature within the vessel.
  • the method comprises controlling the atmospheric pressure within the vessel.
  • the method comprises adding one or more gases to the vessel.
  • the method comprises adding one or more substances selected to simulate a geographic location during maturation.
  • the method comprises maintaining a positive atmospheric pressure within the vessel. Additionally, or alternatively, the method comprises controlling a partial pressure of water vapour within the vessel to control the relative loss of water versus ethanol from the cask.
  • the method comprises periodically purging the vessel. This permits further gas exchange between the cask and the expansion volume in the vessel, most preferably after the equilibrium condition is reached.
  • Embodiments of the sixth aspect of the invention may include one or more features corresponding to features of any of the first to fifth aspects of the invention or its embodiments, or vice versa.
  • a cask leak testing system comprising the apparatus of the first aspect, the system of the third aspect, or the system of the fifth aspect.
  • the system comprises imaging means configured to obtain one or more images of the cask to identify the location and size of one or more leaks in the cask.
  • the imaging means comprises an active infrared hyperspectral imaging system.
  • Embodiments of the seventh aspect of the invention may include one or more features corresponding to features of any of the first to sixth aspects of the invention or its embodiments, or vice versa.
  • a method of testing a cask for leaks comprising sealing the cask within a vessel of the first aspect and employing a monitoring system of the third aspect.
  • the method comprises filling the cask with a test gas, and detecting the presence of the test gas within the expansion volume of the vessel using the monitoring system.
  • Embodiments of the eighth aspect of the invention may include one or more features corresponding to features of any of the first to seventh aspects of the invention or its embodiments, or vice versa.
  • FIG. 1 illustrates in schematic form an apparatus to monitor and control whisky maturation process in accordance with an aspect of the present invention
  • FIG. 2 is a graph of relative transmission of a light beam directed through the apparatus illustrated in FIG. 1 versus time, during the initial stages of a maturation process, in accordance with an aspect of the present invention.
  • FIG. 1 illustrates an apparatus 1 for monitoring and controlling the whisky maturation process, comprising a vessel 3 to house a whisky cask 5 .
  • the vessel 3 is rectangular box, in this embodiment made of aluminium, and comprises a lid 7 to provide access to the vessel.
  • the lid 7 is held in place using screws and has a rubber gasket (not shown) such that when the lid 7 is screwed down the vessel 3 is sealed.
  • the vessel provides an expansion volume (i.e. the internal volume not occupied by the cask 5 ) into which vapour (e.g. ethanol vapour) from the cask may expand. As will be demonstrated below, experimental results show that this prevents further fluid loss from the cask once an equilibrium condition is reached.
  • vapour e.g. ethanol vapour
  • Two apertures 9 a , 9 b are provided at opposing ends of the vessel, defining an optical path through the vessel.
  • the apertures are sealed by way of calcium fluoride (CaF 2 ) windows affixed thereto, although any suitable material for the windows may be used.
  • CaF 2 calcium fluoride
  • an infrared laser source 11 in this example a mid-infrared optical parametric oscillator source outputting 70 mW at approximately 3306 nm (although it will be readily apparent that any other suitable infrared light source may be employed), is directed through the apertures to a detector 13 .
  • This particular wavelength coincides with the O—H and C—H stretch absorption bands of ethanol, and accordingly transmission through the vessel gives an indication of the presence of ethanol within the vessel.
  • the detector 13 in this case a laser power meter, is connected to a data logger (not shown), for example a PC with a suitable data acquisition card, to record transmitted power as a function of time.
  • a background level for determining relative transmission or absorption is obtained without the cask 5 present in the vessel 3 , although the background measurement could be taken immediately after the cask 5 is placed in the vessel 3 (before or after the lid 7 is in place) before any significant ethanol leakage occurs. Subsequently, the lid 7 is secured in place, creating a seal. As noted above, ethanol will leak out of the cask 5 in the form of ethanol vapour, which results in absorption of the laser light within the vessel 3 . This absorption is detected by way of a reduction in optical power through the vessel 3 , detected by the detector 13 .
  • an alternative embodiment of the invention comprises the laser source and power meter housed inside the vessel, in which case the apertures are not required.
  • the monitoring system of the invention may be employed as a stand-alone monitoring system separate from a vessel, and employed to monitor fluid loss from a cask by detecting the presence of, say, ethanol vapour proximal to the cask.
  • FIG. 2 illustrates an exemplary graph 21 of relative transmission 23 as a function of time, illustrating the leak rate of ethanol vapour from a test cask ( 5 ) housed within a vessel.
  • Relative transmission is determined by dividing the measured optical power at time t with the background measurement obtained at the start of the process.
  • a single aperture may be provided with a retro-reflecting mirror inside the vessel—for example on the opposing side of the vessel from the single aperture.
  • the advantage would be two-fold; the absorption pathlength (and hence, sensitivity) would be doubled and the vessel could be monitored from one side.
  • the whisky cask 5 is shown sitting horizontally within the vessel, however it will be understood that the cask 5 may sit vertically or at any other orientation.
  • the vessel 3 is illustrated as being a rectangular box, any other suitable shape of container may be employed. For example, it may be useful to be cylindrical or cask-shaped in order to conform to existing storage facilities.
  • the vessel of this exemplary embodiment has been described as comprising aluminium, any other suitable material may be employed.
  • a vessel may be sized to accommodate multiple whisky casks; a particular advantage being that the maturation process can be monitored and controlled for all said whisky casks at once, thus improving consistency of product between casks.
  • several vessels could be linked by conduits such that conditions are shared throughout, whereupon a single one of said vessels could be monitored as described herein in the knowledge that conditions within or changes made to that vessel will correspond with or result in corresponding changes in conditions in the linked vessels.
  • a spectrometer may be of any suitable kind, for example a tuneable diode laser absorption spectrometer or an active infrared hyperspectral imaging system such as the Applicant's intra-cavity optical parametric oscillator based system.
  • a detailed analysis of the composition of the atmosphere within the vessel might be determined in real-time.
  • the foregoing description of the invention provides an apparatus and a method that first and foremost prevents fluid loss from the cask once an equilibrium position has been reached.
  • the apparatus and method also allows the level of ethanol vapour leaking from the cask to be monitored.
  • the atmospheric composition can also be determined.
  • the cask is also protected from external influences such as airborne pollutants.
  • the invention provides for a system and a method for controlling the maturation process. It has been found that simply sealing casks, for example by shrink-wrapping, does eliminate fluid loss however it also affects the maturation process because ingress of air into the cask from the surroundings is also prevented. This is expected to be of significant detriment to the taste of the whisky—whisky should be allowed to “breathe” as it matures.
  • the vessel provides an expansion volume.
  • environmental conditions within the vessel 3 can be controlled throughout the maturation period.
  • the system comprises a control system that allows the pressure within the vessel 3 to be controlled, as well as the relative humidity and atmospheric composition and of course temperature. This control may comprise maintaining the same environmental conditions throughout an entire maturation process or alternatively varying the environmental conditions as required. By controlling the environmental conditions the maturation process of the whisky can also be controlled.
  • salt water could be injected to simulate the sea air of a shore-side maturation location.
  • control system is used to maintain a small positive atmospheric pressure within the sealed vessel. Accordingly, the fluid loss from the cask resulting from the angels' share is minimised while still allowing for air (oxygen) ingress into the cask to allow the whisky to mature properly.
  • the vessel may be sized to provide sufficient atmospheric oxygen for an entire maturation process or portion thereof.
  • the partial pressure of ethanol within the vessel resulting from the angels' share will plateau over the course of, say, a few days yet proper oxygenation is provided for over the course of a number of years. If necessary, the vessel can be purged and refilled every few years. Even with regular purging, the anticipated loss to the angels' share will be significantly reduced over the entire maturation process.
  • the ratio of water loss to ethanol loss from a cask is dependent on the prevailing atmospheric conditions; principally relative humidity and temperature, although other conditions may also have an effect.
  • higher temperatures are found to increase losses of both ethanol and water.
  • Higher humidity results in increased ethanol loss (relative to water) and lower humidity results in increased water loss (relative to ethanol).
  • the system described herein allows these conditions (temperature and relative humidity) to be controlled, thus controlling the maturation process.
  • this system will be in the event that testing during the maturation process reveals some issue with the whisky that can be remedied by varying the atmospheric conditions. For example, if it was deemed that increased water loss was required, relative humidity could be reduced. In this way, a specific ethanol content can be targeted, particularly during the final stages of the maturation process. This may, for example, be used to increase alcohol content of whisky or to reduce the alcohol content of wine in the final product—as is often required in the industry.
  • a further application of the present invention is to detect leaks in a cask, whereby the cask is inserted into the vessel and leakage into the vessel monitored as a function of time to determine the presence of a leak and quantify the extent of the leak. This is preferably carried out before filling with whisky—for example by filling with a test gas. It is envisaged that imaging systems (such as the applicant's active infrared hyperspectral imaging system) may be employed to identify the location and/or the size of any leaks in the cask.
  • the invention provides an apparatus and a method that reduces fluid loss from a cask during a maturation process by sealably enclosing the cask in a vessel that provides an expansion volume to receive fluid vapour from the cask, a monitoring system and a method that monitors fluid loss from a cask during a maturation process using a light source and a detector to determine the presence of fluid vapour in the vicinity of the cask, a corresponding system for controlling a maturation process in which environmental conditions are controlled, and a cask leak testing system and method making use of the above.

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  • Physics & Mathematics (AREA)
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US14/232,030 2011-07-11 2012-07-10 Maturation apparatus and methods Active US9383314B2 (en)

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Application Number Priority Date Filing Date Title
GB1111837.9A GB2494853B (en) 2011-07-11 2011-07-11 Maturation apparatus and methods
GB1111837.9 2011-07-11
PCT/GB2012/051621 WO2013008003A1 (en) 2011-07-11 2012-07-10 Maturation apparatus and methods

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US20140160465A1 US20140160465A1 (en) 2014-06-12
US9383314B2 true US9383314B2 (en) 2016-07-05

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US (1) US9383314B2 (pt)
EP (1) EP2732019B1 (pt)
JP (1) JP6078061B2 (pt)
CA (1) CA2841215C (pt)
ES (1) ES2558566T3 (pt)
GB (1) GB2494853B (pt)
PL (1) PL2732019T3 (pt)
PT (1) PT2732019E (pt)
WO (1) WO2013008003A1 (pt)

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GB2514387B (en) 2013-05-22 2015-08-12 M Squared Lasers Ltd Maturation monitoring apparatus and methods
US9944891B2 (en) 2013-07-18 2018-04-17 Cryovac, Inc. Process for reducing ethanol loss while developing desirable organoleptics during wooden barrel aging of alcoholic beverage
GB2518147A (en) * 2013-09-10 2015-03-18 M Squared Lasers Ltd Maturation apparatus and monitoring methods
FR3020005B1 (fr) * 2014-04-22 2016-05-13 Pernod Ricard Fut en bois pour le vieillissement d'un spiritueux et procede de vieillissement d'un spiritueux
CN104374729B (zh) * 2014-11-26 2017-07-07 复旦大学 一种实时跟踪一种物质吸收/脱除另外物质全过程的红外检测方法
US11384324B2 (en) 2015-02-24 2022-07-12 Albrecht Holdings Llc Reconditioned or infused fluid containers and related methods
US20150307425A1 (en) * 2015-06-25 2015-10-29 Benjamin Cox Recapture of ethanol from aging barrel
FR3047997B1 (fr) * 2016-02-24 2018-03-30 Renaud Maroy Procede de maturation d'au moins un liquide alcoolise avec recuperation de composes volatils et installation correspondante
SE541253C2 (en) * 2017-10-18 2019-05-14 Gasporox Ab System and method for determining the integrity of containers by optical measurement
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CA2841215C (en) 2019-06-18
JP6078061B2 (ja) 2017-02-08
WO2013008003A1 (en) 2013-01-17
US20140160465A1 (en) 2014-06-12
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GB201111837D0 (en) 2011-08-24
GB2494853B (en) 2013-09-04

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